US9440885B2 - Dielectric ceramic composition and electronic component - Google Patents

Dielectric ceramic composition and electronic component Download PDF

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US9440885B2
US9440885B2 US14/663,160 US201514663160A US9440885B2 US 9440885 B2 US9440885 B2 US 9440885B2 US 201514663160 A US201514663160 A US 201514663160A US 9440885 B2 US9440885 B2 US 9440885B2
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dielectric
segregation
particles
particle
ceramic composition
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US20150274597A1 (en
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Nobuto Morigasaki
Takeru Yoshida
Tomohisa Fukuoka
Yuhta Matsunaga
Kazuhiro Komatsu
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TDK Corp
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Definitions

  • the present invention relates to a dielectric ceramic composition and a ceramic electronic component having a dielectric layer composed of the dielectric ceramic composition.
  • a multilayer ceramic capacitor that is one example of ceramic electronic components is widely used as electronic component having compact size, high efficiency and high reliability.
  • a number of the multilayer ceramic capacitors are particularly used in electric and electronic apparatuses.
  • Patent Document 1 and Patent Document 2 propose multilayer ceramic capacitors to meet such demands.
  • the multilayer ceramic capacitor is further requested to be smaller and achieve higher capacity.
  • dielectric layers are required to be thinner and more multilayered.
  • the present invention has been made by considering such situation, and a purpose of the invention is to provide a dielectric ceramic composition and an electronic component satisfying good temperature characteristics and sufficient reliability even when electric field intensity is increased by making a dielectric layer thinner than before or when the number of the dielectric layers is increased.
  • a dielectric ceramic composition according to the present invention comprises:
  • ABO 3 a main component having perovskite type crystal structure shown by a general formula ABO 3 , where A is at least one selected from the group consisting of Ba, Ca and Sr, and B is at least one selected from the group consisting of Ti and Zr; and
  • the dielectric ceramic composition includes at least dielectric particles having a core-shell structure and segregation particles,
  • a concentration of the rare earth compound in the segregation particle is twice or more than an average concentration of the rare earth compound in a shell part of the dielectric particle having the core-shell structure
  • an area occupied by the segregation particles is 0.1 to 1.1%
  • a maximum particle size of the segregation particle is defined as r bmax
  • a minimum particle size of the segregation particle is defined as r bmin
  • an average particle size of the dielectric particle having the core-shell structure is defined as r a , a relation of r bmax /r a ⁇ 2.00 and r bmin /r a ⁇ 0.25 is satisfied, and
  • the segregation particles substantially do not include Mg.
  • the average particle size r a of the dielectric particle “a” is 0.16 to 0.26 ⁇ m.
  • the dielectric ceramic composition according to the present invention comprises:
  • Ra is at least one selected from the group consisting of Dy, Gd and Tb;
  • the rare earth compound with respect to 100 moles of the main component.
  • the dielectric ceramic composition according to the present invention comprises 0.6 to 1.6 moles of an oxide of Mg in terms of Mg, as the additive, with respect to 100 moles of the main component.
  • the dielectric ceramic composition according to the present invention comprises 0.6 to less than 1.2 moles of a compound including Si in terms of Si, as the additive, with respect to 100 moles of the main component.
  • a ceramic electronic component according to the present invention has a dielectric layer composed of the dielectric ceramic composition, and an electrode layer.
  • FIG. 1 is a cross sectional view of a multilayer ceramic capacitor according to one embodiment of the present invention.
  • FIG. 2 is an enlarged cross sectional view of a main part of dielectric layers 2 shown in FIG. 1 .
  • FIG. 3A is a schematic view of a cut surface of a dielectric ceramic composition according to Sample 3.
  • FIG. 3B is a schematic view of a cut surface of a dielectric ceramic composition according to Sample 16.
  • FIG. 3C is a schematic view of a cut surface of a dielectric ceramic composition according to Sample 21.
  • a multilayer ceramic capacitor 1 as one example of multilayer ceramic electronic components comprises a capacitor element body 10 , where dielectric layers 2 and internal electrode layers 3 are alternately stacked.
  • the internal electrode layers 3 are stacked so that each end face is alternately exposed to surfaces of the two opposed end portions of the capacitor element body 10 .
  • the pair of external electrodes 4 is formed at both end portions of the capacitor element body 10 , and connected with the exposed end faces of the alternately-stacked internal electrode layers 3 to form a capacitor circuit.
  • the capacitor element body 10 is not limited to a particular shape, it is normally formed as a rectangular parallelepiped shape as shown in FIG. 1 . Also, the capacitor element body 10 is not limited to a particular dimension.
  • the dielectric layer 2 is composed of a dielectric ceramic composition according to the present embodiment.
  • the dielectric ceramic composition according to the present embodiment includes, as a main component, a compound shown by a general formula ABO 3 (“A” is at least one selected from Ba, Ca and Sr, and “B” is at least one selected from Ti and Zr). Also, the dielectric ceramic composition includes dielectric particles whose main component is ABO 3 .
  • “x” is preferably 0 ⁇ x ⁇ 0.1, more preferably 0 ⁇ x ⁇ 0.05.
  • temperature characteristic and specific permittivity of the dielectric layers composed of the dielectric ceramic composition according to the present invention can be controlled within a preferable range.
  • “x” is too large, specific permittivity of the dielectric layers tends to be too low.
  • Ca may not be necessarily included. That is, “x” may be zero.
  • “y” is preferably 0 ⁇ y ⁇ 0.1, more preferably 0 ⁇ y ⁇ 0.05.
  • “y” is preferably 0 ⁇ y ⁇ 0.1, more preferably 0 ⁇ y ⁇ 0.05.
  • “z” is preferably 0 ⁇ z ⁇ 0.3, more preferably 0 ⁇ z ⁇ 0.15.
  • “z” is preferably 0 ⁇ z ⁇ 0.3, more preferably 0 ⁇ z ⁇ 0.15.
  • the dielectric ceramic composition according to the present embodiment includes at least a rare earth compound as the additive.
  • the rare earth compound all of an oxide of Ra, an oxide of Rb and an oxide of Rc are preferably included.
  • Ra is at least one selected from a group of Dy, Gd and Tb.
  • Rb is at least one selected from a group of Ho and Y.
  • Rc is at least one selected from a group of Yb and Lu.
  • ⁇ is preferably 0.6 to 1.4 moles, more preferably 0.7 to 1.2 moles in terms of Ra 2 O 3 .
  • ⁇ is particularly preferable to use Dy as the oxide of Ra.
  • ⁇ is preferably 0.2 to 0.7 mole, more preferably 0.2 to 0.6 mole in terms of Rb 2 O 3 .
  • ⁇ is particularly preferable to include Ho as the oxide of Rb.
  • ⁇ is preferably 0.2 to 0.7 mole, more preferably 0.2 to 0.5 mole in terms of Rc 2 O 3 .
  • ⁇ is particularly preferable to include Yb as the oxide of Rc.
  • specific rare earth elements are divided into Ra, Rb and Rc based on values of effective ionic radius for six-fold coordination.
  • effective ionic radius when the difference between the rare earth elements and the Ba site atom is small, they tend to easily substitute (be solid-soluted into) A site, and when the difference between the rare earth elements and the Ba site atom is large, they tend to be hard to substitute (be solid-soluted into) A site.
  • the rare earth elements having a small ionic radius difference from Ba site atom correspond with Ra
  • the rare earth elements having a large ionic radius difference from Ba correspond with Rc
  • Ra and Rc are different in the degree of solute into ABO 3 .
  • Ra tends to easily be solid-soluted into ABO 3 totally
  • Rc tends to be solid-soluted into only periphery of ABO 3 and to form so-called core-shell structure.
  • addition of Ra to the dielectric ceramic composition improves high temperature accelerated lifetime thereof, but temperature characteristic tends to be deteriorated.
  • addition of Rc to the dielectric ceramic composition improves temperature characteristic thereof, but high temperature accelerated lifetime tends to be deteriorated.
  • Rb has ionic radius difference from Ba site atom which is approximately between Ra and Rc.
  • the contents of the group of the three kinds of the rare earth elements of Ra, Rb and Rc are adjusted, which makes it easier to further improve high temperature accelerated lifetime while controlling the degree of solute rare earth elements of Ra, Rb and Rc and maintaining a preferable temperature characteristic.
  • the dielectric ceramic composition further include an oxide of Mg.
  • the content of an oxide of Mg is preferably 0.6 to 1.2 moles, more preferably 0.7 to 1.1 moles in terms of MgO.
  • Mg-including segregation particles mentioned below are hard to be present.
  • the content of the oxide of Mg the lower limit or more of the above value range abnormal grain growth of the dielectric particles is effectively prevented. Note that, when the dielectric particles abnormally grain grow and average particle size of the dielectric particles “a” having core-shell structure becomes too large, temperature characteristic of the dielectric layers tends to be deteriorated.
  • the dielectric ceramic composition further include a compound including Si.
  • the compound including Si is preferably an oxide of Si.
  • the oxide of Si mainly has a role as a sintering aid.
  • a content of the oxide of Si is preferably 0.6 to less than 1.2 moles, more preferably 0.8 to 1.1 moles in terms of SiO 2 .
  • the dielectric ceramic composition according to the present embodiment preferably further includes, as the additive, at least one or more oxides selected from a group of V, Mo and W and an oxide of Mn and/or Cr.
  • at least one or more oxides selected from a group of V, Mo and W and an oxide of Mn and/or Cr By including the above components, characteristic can be further improved.
  • a content of at least one or more oxides selected from a group of V, Mo and W is preferably 0.03 to 0.1 mole and more preferably 0.05 to 0.09 mole in terms of V, Mo and W.
  • a content of the oxide of Mn and/or Cr is preferably 0.10 to 0.20 mole in terms of Mn and/or Cr.
  • oxides include “composite oxides”.
  • the dielectric layer of the present embodiment is not limited to a particular thickness, but it is preferably 1.0 to 10.0 ⁇ m.
  • stacked layers of the dielectric layer is not limited to a particular number, the number is preferably 20 or more, more preferably 50 or more, and still more preferably 100 or more. Although not particularly limited, an upper limit of the number of stacked layers is, for example, 2000 and so on.
  • dielectric particles “a” and the segregation particle “b” are present as sub components in the ABO 3 particle which is the main component.
  • the dielectric particles “a” have core-shell structure where at least rare earth oxide is solid-soluted.
  • the segregation particle “b” includes rare earth oxide at a high concentration.
  • other dielectric particle “c”, which corresponds with neither the dielectric particles “a” having the above core-shell structure nor the segregation particle “b”, may be present.
  • the dielectric particle “a” having core-shell structure is defined as a particle whose contrast is different between central part and peripheral part when reflected electron image of cut surface is photographed by Field Emission Scanning Electron Microscope (FE-SEM). Then, as shown in FIG. 2 , the central part and the peripheral part of the dielectric particle “a” are defined as a core part a 1 and a shell part a 2 , respectively.
  • FE-SEM Field Emission Scanning Electron Microscope
  • the segregation particle “b” is a particle whose concentration of rare earth oxide is twice or more in the whole area thereof than average concentration of rare earth oxide of the shell part a 2 of the dielectric particle “a” having core-shell structure. In the reflected electron image, the segregation particle “b” has contrast different from that of the core part a 1 and the shell part a 2 .
  • a method for measuring particle size and existing area of dielectric particles included in a dielectric layer is not limited, and they are measured by the following method, for example.
  • the number of pictures, observation area and magnification of the reflected electron image is not limited, but the reflected electron image is preferably photographed (multiple times) so that approximately 1000 or more of the dielectric particles “a” having core-shell structure are included in total.
  • the magnification is preferably around 20000.
  • the reflected electron image is processed by image processing software, and particle size and existing area are calculated by assuming that the shapes of the dielectric particles are sphere.
  • An average particle size r a of the dielectric particles “a” having core-shell structure is preferably calculated by averaging particle sizes of the dielectric particles “a” having approximately 1000 or more core-shell structures.
  • a maximum particle size r bmax of the segregation particle “b” and a minimum particle size r bmin thereof are determined by measuring particle sizes of all of the segregation particles “b” present in the photographed reflected electron image.
  • a method for confirming the presence of Mg in the segregation particles “b” included in the dielectric layer is not limited, but it can be confirmed by the following method, for example.
  • Mapping images of rare earth elements are formed by using STEM-EDX, and the segregation particles “b” are visually determined. Then, concentration of Mg is measured by point analysis of STEM-EDX against all of the segregation particles “b” determined visually, which confirms the presence of Mg in the segregation particles “b”.
  • segregation particles substantially including Mg may be referred as Mg-including segregation particles.
  • the average particle size r a of the dielectric particles “a” having core-shell structures is preferably 0.16 to 0.26 ⁇ m, more preferably 0.17 to 0.25 ⁇ m.
  • r bmax /r a ⁇ 2.0 is satisfied by the relation between the maximum particle size r bmax of the segregation particles “b” and the average particle size r a of the dielectric particles “a” having core-shell structures.
  • r bmax /r a ⁇ 1.8 is satisfied.
  • r bmin /r a ⁇ 0.25 is satisfied by the relation between the minimum particle size r bmin of the segregation particles “b” and the average particle size r a of the dielectric particles “a” having core-shell structures.
  • r bmin /r a ⁇ 0.40 is satisfied.
  • r bmin is too small for r a or the segregation particle “b” is not present, high temperature accelerated lifetime is decreased. This is because additives are not adequately solid-soluted in the dielectric particles “a”.
  • Mg is easily included in the segregation particles “b” whose particle size is small.
  • the dielectric ceramic composition according to the present embodiment does not include the segregation particle “b” substantially including Mg. That is, in the present embodiment, the segregation particle “b” detected by observing the dielectric layer does not include Mg substantially. When the segregation particle “b” substantially including Mg is present, high temperature accelerated lifetime is extremely decreased.
  • an area of an existing region of the dielectric particles “a” having core-shell structures is preferably 60% or more, more preferably 70% or more.
  • an area of an existing region of the segregation particles “b” is 0.1 to 1.1%.
  • the total area is 0.3 to 0.5%.
  • components constituting the segregation particle “b” of the present embodiment be substantially made of R—Si—Ba—Ti—O composite oxide.
  • the other dielectric particle “c” is not limited to a particular embodiment.
  • a low-concentration complete solid-soluted particle whose contrast is similar to that of the shell part of the dielectric particle “a” having core-shell structure, an ABO 3 particle where additives are not solid-soluted at all, and a dielectric particle where only additives other than the rare earth elements are solid-soluted are exemplified.
  • existence probability of the other dielectric particle “c” may be 0%, that is, particles in the dielectric layer according to the present embodiment may be only the dielectric particles “a” having core-shell structures and the segregation particles “b” not substantially including Mg.
  • the dielectric particles “a” having core-shell structures and the other dielectric particle “c” may include Mg or may not include Mg.
  • a conductive material included in the internal electrode layer 3 is not limited. However, comparatively inexpensive base metal may be used because the material constituting the dielectric layer has resistance to reduction.
  • Ni or Ni alloy is preferable.
  • the Ni alloy an alloy of Ni and one or more kind elements selected from Mn, Cr, Co and Al is preferable.
  • Ni content in the alloy is preferably 95 wt % or more.
  • 0.1 wt % or below or so of various miner components such as P may be included in the Ni or Ni alloy.
  • a thickness of the internal electrode layer 3 may be suitably changed depending on a purpose of use, and is not limited. It is normally 0.1 to 3.0 ⁇ M and preferably 0.5 to 2.0 ⁇ m or so.
  • a conductive material included in external electrodes 4 is not limited, in the present embodiment, inexpensive Ni, Cu and their alloys may be used.
  • a thickness of the external electrode 4 may be suitably determined depending on a purpose of use and the like, but it is normally preferably 10 to 50 ⁇ m or so.
  • the multilayer ceramic capacitor 1 of the present embodiment is produced by producing green chips with normal printing method or sheet method using a paste, firing them, and firing external electrodes after printing or transferring them.
  • a producing method will be explained specifically.
  • dielectric material (dielectric ceramic composition powder) is prepared and made into paste to prepare a paste (dielectric layer paste) for forming the dielectric layer.
  • the main component material of the dielectric material firstly, a material of ABO 3 is prepared. It is preferable to use barium titanate shown by Ba u Ti v O 3 as ABO 3 .
  • the material of the ABO 3 may be one produced by various methods such as various liquid phase methods (for example, oxalate method, hydrothermal synthesis method, alkoxide method, sol-gel method and the like) as well as so-called solid phase method.
  • various liquid phase methods for example, oxalate method, hydrothermal synthesis method, alkoxide method, sol-gel method and the like
  • u/v is preferably within a range of 1.000 ⁇ u/v ⁇ 1.005. By setting u/v within the above range, it becomes easier to favorably control grain growth during firing. Then, temperature characteristic and high temperature accelerated lifetime are improved.
  • an average particle size of the material of barium titanate is not limited, but it is preferably 0.13 to 0.23 ⁇ m and more preferably 0.16 to 0.22 ⁇ m.
  • an average particle size of barium titanate used within the above range it becomes easier to preferably control sintering and grain growth of the segregation particle “b”. Then, reliability and temperature characteristic are improved.
  • oxide of the above mentioned component can be used.
  • various compounds to be the above oxide or composite oxide by firing can be used.
  • a compound can be used by suitably selecting from such as carbonate, oxalate, nitrate, hydroxide or organic metal compounds and mixing it.
  • the producing method for the above dielectric ceramic composition powder is not limited, and as a method other than the above, barium titanate powder may be coated with a sub component, for example.
  • the sub component for coating is not limited to a particular kind, either, but it is preferably oxide of R (Ra, Rb, Rc), oxide of Mg, and oxide of Si.
  • a known method may be applied to the coating method.
  • barium titanate particle surface can be coated with each sub component by turning oxide of R (Ra, Rb, Rc), oxide of Mg, and oxide of Si into solution, mixing them with slurry in which barium titanate is dispersed, and applying heat treatment thereto.
  • a content of each compound in the dielectric material may be determined to obtain composition of the above-mentioned dielectric ceramic composition after firing. Note that, in the present embodiment, the present inventors confirm that the composition of the dielectric ceramic composition does not substantially change before and after firing except for a special case such as one that a part of each sub component mentioned above is vaporized during firing.
  • the dielectric layer paste may be an organic type paste obtained by kneading the dielectric material and an organic vehicle, or may be a water-based paste obtained by kneading the dielectric material and a water-based vehicle.
  • the organic vehicle is obtained by dissolving a binder in an organic solvent.
  • the binder is not limited, and may be suitably selected from various binders for a normal organic vehicle such as ethyl cellulose, polyvinyl butyral and the like.
  • the organic solvent to be used is not limited, and may be suitably selected from various organic solvents such as terpineol, butyl carbitol, acetone, toluene and the like depending on the method to be used such as printing method or sheet method.
  • the water-based vehicle is obtained by dissolving a water soluble binder or dispersion agent etc. in water.
  • the water soluble binder for the water-based vehicle is not limited, and may be suitably selected from various normal binders for a normal water-based vehicle such as polyvinyl alcohol, cellulose, water-soluble acrylic resin and the like.
  • An internal electrode layer paste is obtained by kneading the above-mentioned organic vehicle and conductive materials composed of the above-mentioned various conductive metals or alloys, or various oxides, organic metallic compound and resinate etc. to be the above-mentioned conductive materials after firing.
  • the internal electrode layer paste may include an inhibitor.
  • the inhibitor is not limited, but preferably includes barium titanate.
  • the external electrode paste may be prepared in the same way as the above-mentioned internal electrode layer paste.
  • the organic vehicle in each of the above mentioned paste is not limited to a particular content, and may be normal content.
  • a content of the binder may be 1 to 10 wt % or so
  • a content of the solvent may be 10 to 50 wt % or so.
  • additives selected from various dispersant agent, plasticizer, dielectric material, insulation material and the like may be included if needed.
  • a total amount thereof is preferably 10 wt % or less.
  • the dielectric layer paste and the internal electrode layer paste are printed, stacked on a substrate such as PET and cut in a predetermined shape. Then, green chip is obtained by removing from the substrate.
  • a green sheet is formed by using the dielectric layer paste, and the internal electrode layer paste is printed thereon to form internal electrode patterns. Then, a green chip is obtained by stacking them.
  • the binder removal conditions are not limited, but a temperature rising rate is preferably 5 to 300° C./hr; a holding temperature is preferably 180 to 800° C., and a temperature holding time is preferably 0.5 to 48 hrs. Also, binder removal atmosphere is preferably air or reducing atmosphere.
  • a temperature rising rate is preferably 100 to 2000° C./hr, more preferably 600 to 1000° C./hr.
  • a holding temperature during firing is preferably 1300° C. or less, more preferably 1180 to 1290° C.
  • a holding time during firing is preferably 0.2 to 20 hrs, more preferably 0.5 to 15 hrs.
  • Firing atmosphere is preferably reducing atmosphere.
  • An atmosphere gas is not limited and, for example, a wet mixture gas of N 2 and H 2 may be used.
  • an oxygen partial pressure during firing may be suitably determined depending on a kind of the conductive material in the internal electrode layer paste.
  • the oxygen partial pressure in the firing atmosphere is preferably 10 ⁇ 14 to 10 ⁇ 10 MPa.
  • the annealing is a treatment for reoxidation of the dielectric layer.
  • the annealing enables insulation resistance (IR) of the dielectric layer to be improved remarkably and also enables high temperature accelerated lifetime (IR lifetime) to be improved.
  • the atmosphere during the annealing is not limited, but an oxygen partial pressure is preferably 10 ⁇ 9 to 10 ⁇ 5 MPa. By setting the oxygen partial pressure within the range, reoxidation of the dielectric layer becomes easier while the internal electrode layer is prevented from oxidizing.
  • a holding temperature during the annealing is not particularly limited, but it is preferably 1100° C. or less and more preferably 950 to 1090° C.
  • the dielectric layer is easy to be oxidized sufficiently. Also, oxidization of the internal electrode layer and reaction between the internal electrode layer and the dielectric layer are prevented, and temperature characteristic of the dielectric layer, insulation resistance (IR), high temperature accelerated lifetime (IR lifetime) and capacitance of a capacitor tend to be favorable.
  • a temperature holding time is preferably 0 to 20 hrs, more preferably 2 to 4 hrs.
  • a temperature descending rate is preferably 50 to 1000° C./hr, more preferably 100 to 600° C./hr.
  • an atmosphere gas of the annealing is not limited and, for example, a wet N 2 gas is preferably used.
  • a wetter or so may be used to wet the N 2 gas, mixture gas and the like.
  • a water temperature is preferably 5 to 75° C. or so.
  • the binder removal treatment, firing and annealing may be performed continuously or individually.
  • BaCO 3 powder was prepared as oxide material of Ba
  • MgO powder was prepared as oxide material of Mg
  • MnCO 3 powder was prepared as oxide material of Mn
  • V 2 O 5 powder was prepared as oxide material of V
  • SiO 2 powder was prepared as a sintering aid.
  • dielectric layer paste 100 parts by weight of the obtained dielectric material, 10 parts by weight of polyvinyl butyral resin, 5 parts by weight of dioctylphthalate (DOP) as a plasticizer, and 100 parts by weight of alcohol as solvent were mixed by a ball mill and made into a paste, so that a dielectric layer paste was obtained.
  • DOP dioctylphthalate
  • a green sheet was formed on a PET film by using the dielectric layer paste prepared in the above procedure so that thickness of the green sheet was 4.5 ⁇ m after drying.
  • a sheet was removed from the PET film, so that a green sheet having the electrode layer was made.
  • a plurality of green sheets having the electrode layer was stacked and adhered by pressure to form a green stacking body. The green stacking body was cut in a predetermined size to obtain a green chip.
  • the obtained green chip was subject to binder removal treatment, firing and annealing under the following conditions, so that a multilayer ceramic firing body was obtained.
  • the binder removal treatment was performed under the following conditions: temperature rising rate was 25° C./hr; holding temperature was 235° C.; holding time was 8 hrs; and atmosphere was in the air.
  • the firing was performed under the following conditions: temperature rising rate was 200° C./hr; holding temperature was 1260° C.; and holding time was 2 hrs. A temperature descending rate was 200° C./hr. Note that, an atmosphere gas was wet N 2 +H 2 mixture gas so that an oxygen partial pressure was adjusted to 10 ⁇ 12 MPa.
  • the annealing was performed under the following conditions: temperature rising rate was 200° C./hr; holding temperature was 1050° C.; holding time was 3 hrs; temperature descending rate was 200° C./hr; and atmosphere gas was wet N 2 gas (oxygen partial pressure: 10 ⁇ 7 MPa).
  • multilayer ceramic capacitor Samples 1 to 8 shown in Table. 1 were obtained (hereinafter, they may be merely represented as “capacitor samples”).
  • the size of the obtained capacitor samples was 3.2 mm ⁇ 1.6 mm ⁇ 1.2 mm, the thickness between the adjacent dielectric layers was 3.0 ⁇ m, the thickness of the internal electrode layer was 1.0 ⁇ m.
  • the number of the dielectric layers was 200.
  • each capacitor sample As for the obtained each capacitor sample, the following measurement and confirmation were respectively performed by the method mentioned below.
  • the measurement was carried out for specific permittivity; temperature characteristics, high temperature accelerated lifetime (HALT), average particle sizes r a of the dielectric particle “a” having core-shell structures, the maximum particle size r bmax of the segregation particles “b”, and the minimum particle size r bmin of the segregation particles “b”.
  • the confirmation was carried out for existence of Mg in the segregation particle “b”. The results are shown in Table 1.
  • Specific permittivity of the capacitor samples was measured at a reference temperature of 25° C. with a digital LCR meter (4274A made by YHP) under conditions of a frequency of 1.0 kHz and an input signal level (measurement voltage) of 1.0 Vrms. Heat treatment was performed for the capacitor samples at 150° C. for 1 hr., and specific permittivity (no unit) was calculated from capacitance value, thickness of the dielectric body, and overlapping area of the internal electrodes in 24 hours. Higher specific permittivity was preferable, and in the present example, samples whose specific permittivity was 2200 or higher were considered to be favorable.
  • a capacitance from ⁇ 55 to 125° C. was measured under conditions of a frequency of 1.0 kHz and an input signal level (measurement voltage) of 1.0 Vrms, and a change rate of the capacitance was calculated based on the capacitance at 25° C. Then, the change rate was evaluated whether it satisfied the X7R characteristic, which is the temperature characteristic of EIA standard, or not.
  • the lifetime was evaluated by measuring the insulation deterioration time of the capacitor samples while applying the DC voltage under the electric field of 25 V/ ⁇ m at 175° C.
  • the lifetime was defined as the time from the beginning of the voltage application until the insulation resistance dropped by one digit.
  • this high temperature accelerated lifetime evaluation was performed to 20 capacitor samples, and mean time to failure (MTTF), which was calculated by Weibull analysis thereto, was defined as an average lifetime of the samples.
  • MTTF mean time to failure
  • the obtained capacitor samples were cut at a surface vertical to the internal electrodes, and the cut surface was polished. Then, etching treatment was performed for the polished surface by ion milling, and thereafter, reflected electron images in an observation visual field of 3.0 ⁇ 4.0 ⁇ m were photographed by Field Emission Scanning Electron Microscope (FE-SEM). Five reflected electron images were photographed at positions different from each other on the cut surface. In terms of the photographs of the reflected electron images, a dielectric particle whose contrast is different between a central part and a periphery of the particle was considered to be one having core-shell structure.
  • a particle whose contrast was clearly different between the core part and the shell part (contrast which is different from that of the internal electrodes) in the reflected electron images was considered to be a segregation particle.
  • mapping of rare earth elements was performed by Scanning Transmission Electron Microscope Energy Dispersive X-ray (STEM-EDX) belonged to STEM, so that mapping images were made. Then, in the mapping images, contrasts were visually compared as similarly to the reflected electron images, and the dielectric particles having core-shell structures and the segregation particles were determined.
  • shapes of particles were assumed as sphere by image processing software, and in the five photographs of the reflected electron image, an area of segregation particles, an area of dielectric particles having core-shell structure and an area of other dielectric particles were respectively calculated. Then, a segregation particle existing rate was calculated. Also, the maximum particle size r bmax and the minimum particle size r bmin were calculated by assuming that, in terms of multiple segregation particles in the five photographs of the reflected electron image, the segregation particle having the largest particle size and the segregation particle having the smallest particle size have shapes of sphere by image processing software.
  • the polished surface was observed by STEM. This observation was performed in an observation visual field of 1.0 ⁇ 1.0 ⁇ m. Then, mapping of each additive element was performed by Scanning Transmission Electron Microscope Energy Dispersive X-ray (STEM-EDX) belonged to STEM.
  • STEM-EDX Scanning Transmission Electron Microscope Energy Dispersive X-ray
  • Example 3 multilayer ceramic capacitor samples of Samples 14 to 27 were prepared as similar to Sample 3 of Example 1 and characteristic evaluation was performed in the same way as Example 1.
  • the firing conditions of Example 3 were changed as follows: temperature rising rate was 200 to 2000° C./hr; holding temperature was 1180 to 1300° C.; holding time was 0.5 to 20 hrs; and temperature descending rate was 600 to 800° C./hr. Also, an atmosphere gas was wet N 2 +H 2 mixture gas, and an oxygen partial pressure was 10 ⁇ 12 MPa. The results are shown in Table 3.
  • FIG. 3A , FIG. 3B and FIG. 3C show schematic views of the dielectric ceramic compositions regarding Sample 3 (Example), Sample 16 (Comparative Example) and Sample 21 (Example). Note that, in order to prioritize easy understanding, the number of segregation particles “b” and other dielectric particles “c” is described more than the number actually included.
  • FIG. 3B showing Sample 16 is compared with FIG. 3A showing Sample 3 and FIG. 3C showing Sample 21.
  • the dielectric particles “a” having core-shell structure, the segregation particles “b” and the other dielectric particles “c” are commonly observed.
  • FIG. 3B is different from FIG. 3A and FIG. 3C in that minor segregation particles “b” are observed in FIG. 3B , but they are not observed in FIG. 3A and FIG. 3C .
  • r bmin /r a becomes small.
  • the minor segregation particles “b” are mostly Mg-including segregation particles.
  • Mg-including segregation particles are present in the minor segregation particles “b”.

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